# Electronic Supplementary Material (ESI) for Organic .
# This journal is © The Royal Society of Chemistry 2014


data_04171a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H24 O3'
_chemical_formula_weight         408.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   p_1_21/c_1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.1157(3)
_cell_length_b                   21.1608(4)
_cell_length_c                   10.7272(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.050(3)
_cell_angle_gamma                90.00
_cell_volume                     2062.95(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8780
_exptl_absorpt_correction_T_max  0.9362
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12180
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.18
_diffrn_reflns_theta_max         66.85
_reflns_number_total             3647
_reflns_number_gt                3168
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.4655P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0003(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3647
_refine_ls_number_parameters     281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1116
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_restrained_S_all      0.873
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.28087(13) 0.57177(6) 0.16047(13) 0.0225(3) Uani 1 1 d . . .
C17 C 0.36380(14) 0.69731(6) 0.13396(13) 0.0225(3) Uani 1 1 d . . .
H17 H 0.4407 0.7248 0.1318 0.027 Uiso 1 1 calc R . .
C15 C 0.23323(14) 0.61322(6) 0.34560(14) 0.0250(3) Uani 1 1 d . . .
H15 H 0.2498 0.6431 0.4145 0.030 Uiso 1 1 calc R . .
C22 C 0.48863(14) 0.70608(6) 0.40496(13) 0.0236(3) Uani 1 1 d . . .
C10 C 0.31298(13) 0.61551(6) 0.26786(13) 0.0211(3) Uani 1 1 d . . .
C6 C 0.53127(14) 0.58011(6) 0.16498(14) 0.0256(3) Uani 1 1 d . . .
H6 H 0.5804 0.5926 0.1078 0.031 Uiso 1 1 calc R . .
C12 C 0.17645(14) 0.52486(6) 0.13610(14) 0.0267(3) Uani 1 1 d . . .
H12 H 0.1568 0.4957 0.0652 0.032 Uiso 1 1 calc R . .
C16 C 0.32349(15) 0.64851(6) 0.01338(13) 0.0246(3) Uani 1 1 d . . .
H16 H 0.3867 0.6578 -0.0321 0.030 Uiso 1 1 calc R . .
C21 C 0.16595(16) 0.65026(7) -0.09846(14) 0.0306(3) Uani 1 1 d . . .
C18 C 0.23930(15) 0.73978(6) 0.12576(14) 0.0275(3) Uani 1 1 d . . .
C7 C 0.57275(14) 0.62826(6) 0.28712(13) 0.0234(3) Uani 1 1 d . . .
H7 H 0.6400 0.6599 0.2801 0.028 Uiso 1 1 calc R . .
C9 C 0.43082(13) 0.66293(6) 0.27710(12) 0.0208(3) Uani 1 1 d . . .
C24 C 0.57925(17) 0.80814(7) 0.33192(15) 0.0316(3) Uani 1 1 d . . .
H24 H 0.4970 0.8089 0.2463 0.038 Uiso 1 1 calc R . .
C28 C 0.71904(16) 0.76061(7) 0.55434(16) 0.0349(3) Uani 1 1 d . . .
H28 H 0.7305 0.7292 0.6189 0.042 Uiso 1 1 calc R . .
C14 C 0.12849(14) 0.56596(7) 0.31968(14) 0.0296(3) Uani 1 1 d . . .
H14 H 0.0760 0.5644 0.3723 0.036 Uiso 1 1 calc R . .
C23 C 0.59615(15) 0.75962(6) 0.42470(14) 0.0258(3) Uani 1 1 d . . .
C8 C 0.36385(14) 0.58123(6) 0.07516(13) 0.0243(3) Uani 1 1 d . . .
H8 H 0.3348 0.5496 0.0012 0.029 Uiso 1 1 calc R . .
C3 C 0.65881(15) 0.58686(7) 0.41662(14) 0.0302(3) Uani 1 1 d . . .
H3 H 0.6651 0.6041 0.5039 0.036 Uiso 1 1 calc R . .
C4 C 0.58445(15) 0.52189(7) 0.37613(15) 0.0318(3) Uani 1 1 d . . .
H4A H 0.6386 0.4890 0.4416 0.038 Uiso 1 1 calc R . .
H4B H 0.4828 0.5224 0.3616 0.038 Uiso 1 1 calc R . .
C13 C 0.10128(15) 0.52138(7) 0.21749(15) 0.0308(3) Uani 1 1 d . . .
H13 H 0.0333 0.4893 0.2032 0.037 Uiso 1 1 calc R . .
C5 C 0.59941(15) 0.51778(7) 0.24023(16) 0.0316(3) Uani 1 1 d . . .
H5 H 0.5577 0.4795 0.1857 0.038 Uiso 1 1 calc R . .
C19 C 0.10741(17) 0.74702(8) -0.00628(16) 0.0372(4) Uani 1 1 d . . .
H19 H 0.0457 0.7814 -0.0185 0.045 Uiso 1 1 calc R . .
C25 C 0.68433(18) 0.85569(7) 0.36578(16) 0.0364(4) Uani 1 1 d . . .
H25 H 0.6721 0.8879 0.3027 0.044 Uiso 1 1 calc R . .
C27 C 0.82381(17) 0.80796(8) 0.58757(18) 0.0432(4) Uani 1 1 d . . .
H27 H 0.9054 0.8078 0.6737 0.052 Uiso 1 1 calc R . .
C2 C 0.80854(16) 0.57246(8) 0.41644(17) 0.0376(4) Uani 1 1 d . . .
H2A H 0.8770 0.5541 0.5040 0.045 Uiso 1 1 calc R . .
H2B H 0.8517 0.6104 0.3991 0.045 Uiso 1 1 calc R . .
C1 C 0.76768(17) 0.52438(8) 0.29589(18) 0.0396(4) Uani 1 1 d . . .
H1A H 0.7936 0.5404 0.2248 0.047 Uiso 1 1 calc R . .
H1B H 0.8166 0.4842 0.3293 0.047 Uiso 1 1 calc R . .
C26 C 0.80746(17) 0.85523(7) 0.49343(18) 0.0391(4) Uani 1 1 d . . .
H26 H 0.8785 0.8866 0.5153 0.047 Uiso 1 1 calc R . .
C20 C 0.07375(17) 0.70566(8) -0.10899(16) 0.0381(4) Uani 1 1 d . . .
H20 H -0.0114 0.7120 -0.1907 0.046 Uiso 1 1 calc R . .
O2 O 0.24972(12) 0.76858(5) 0.22807(11) 0.0372(3) Uani 1 1 d . . .
O1 O 0.11492(13) 0.60704(5) -0.18015(11) 0.0451(3) Uani 1 1 d . . .
O3 O 0.47051(11) 0.69131(5) 0.50598(10) 0.0317(3) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 C12 1.3881(18) . ?
C11 C10 1.4003(18) . ?
C11 C8 1.5023(18) . ?
C17 C18 1.5180(19) . ?
C17 C9 1.5597(17) . ?
C17 C16 1.5629(17) . ?
C15 C10 1.3927(18) . ?
C15 C14 1.393(2) . ?
C22 O3 1.2166(16) . ?
C22 C23 1.5196(18) . ?
C22 C9 1.5337(17) . ?
C10 C9 1.5276(17) . ?
C6 C8 1.5375(18) . ?
C6 C5 1.542(2) . ?
C6 C7 1.5647(17) . ?
C12 C13 1.389(2) . ?
C16 C21 1.5170(19) . ?
C16 C8 1.5474(18) . ?
C21 O1 1.2139(18) . ?
C21 C20 1.471(2) . ?
C18 O2 1.2187(17) . ?
C18 C19 1.466(2) . ?
C7 C3 1.5470(19) . ?
C7 C9 1.5734(17) . ?
C24 C23 1.387(2) . ?
C24 C25 1.391(2) . ?
C28 C27 1.387(2) . ?
C28 C23 1.401(2) . ?
C14 C13 1.379(2) . ?
C3 C4 1.535(2) . ?
C3 C2 1.546(2) . ?
C4 C5 1.533(2) . ?
C5 C1 1.543(2) . ?
C19 C20 1.329(2) . ?
C25 C26 1.389(2) . ?
C27 C26 1.379(2) . ?
C2 C1 1.552(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 C11 C10 120.67(12) . . ?
C12 C11 C8 124.28(12) . . ?
C10 C11 C8 115.04(11) . . ?
C18 C17 C9 108.91(10) . . ?
C18 C17 C16 115.79(11) . . ?
C9 C17 C16 110.43(10) . . ?
C10 C15 C14 119.68(12) . . ?
O3 C22 C23 116.48(11) . . ?
O3 C22 C9 119.75(11) . . ?
C23 C22 C9 122.48(11) . . ?
C15 C10 C11 118.91(11) . . ?
C15 C10 C9 128.66(11) . . ?
C11 C10 C9 112.34(10) . . ?
C8 C6 C5 117.22(11) . . ?
C8 C6 C7 109.34(10) . . ?
C5 C6 C7 102.99(10) . . ?
C11 C12 C13 120.06(13) . . ?
C21 C16 C8 110.44(10) . . ?
C21 C16 C17 116.10(11) . . ?
C8 C16 C17 109.25(10) . . ?
O1 C21 C20 119.39(13) . . ?
O1 C21 C16 121.23(14) . . ?
C20 C21 C16 119.38(12) . . ?
O2 C18 C19 120.00(13) . . ?
O2 C18 C17 120.16(12) . . ?
C19 C18 C17 119.84(12) . . ?
C3 C7 C6 102.79(11) . . ?
C3 C7 C9 117.53(10) . . ?
C6 C7 C9 110.20(10) . . ?
C10 C9 C22 115.42(10) . . ?
C10 C9 C17 104.66(9) . . ?
C22 C9 C17 115.65(10) . . ?
C10 C9 C7 111.15(10) . . ?
C22 C9 C7 103.79(10) . . ?
C17 C9 C7 105.89(9) . . ?
C23 C24 C25 120.58(14) . . ?
C27 C28 C23 120.73(14) . . ?
C13 C14 C15 121.23(12) . . ?
C24 C23 C28 118.51(13) . . ?
C24 C23 C22 126.64(12) . . ?
C28 C23 C22 114.73(12) . . ?
C11 C8 C6 111.87(10) . . ?
C11 C8 C16 105.70(10) . . ?
C6 C8 C16 107.07(10) . . ?
C4 C3 C2 100.47(12) . . ?
C4 C3 C7 103.92(11) . . ?
C2 C3 C7 106.01(11) . . ?
C5 C4 C3 94.54(11) . . ?
C14 C13 C12 119.35(12) . . ?
C4 C5 C6 103.96(11) . . ?
C4 C5 C1 100.35(12) . . ?
C6 C5 C1 106.79(12) . . ?
C20 C19 C18 121.69(14) . . ?
C26 C25 C24 120.26(14) . . ?
C26 C27 C28 120.24(14) . . ?
C3 C2 C1 103.16(11) . . ?
C5 C1 C2 103.10(11) . . ?
C27 C26 C25 119.64(14) . . ?
C19 C20 C21 122.55(13) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        66.85
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.038
_database_code_depnum_ccdc_archive 'CCDC 983251'

data_04181m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H22 O3'
_chemical_formula_weight         406.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.1109(16)
_cell_length_b                   12.2037(16)
_cell_length_c                   13.4259(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.302(2)
_cell_angle_gamma                90.00
_cell_volume                     1983.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9827
_exptl_absorpt_correction_T_max  0.9913
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9891
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         27.06
_reflns_number_total             4294
_reflns_number_gt                3287
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0628P)²+0.5910P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4294
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1173
_refine_ls_wR_factor_gt          0.1055
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O 0.95734(9) 0.35999(9) 1.02393(8) 0.0295(3) Uani 1 1 d . . .
O1 O 0.96993(9) 0.21885(10) 0.64961(8) 0.0317(3) Uani 1 1 d . . .
O3 O 0.80388(10) 0.18236(9) 1.13759(8) 0.0327(3) Uani 1 1 d . . .
C25 C 0.88590(11) 0.20731(12) 0.80584(10) 0.0213(3) Uani 1 1 d . . .
C9 C 0.68211(11) 0.18074(11) 0.89793(10) 0.0200(3) Uani 1 1 d . . .
C8 C 0.78947(11) 0.18796(11) 0.96063(10) 0.0191(3) Uani 1 1 d . . .
C24 C 0.87554(11) 0.24764(11) 0.89843(10) 0.0201(3) Uani 1 1 d . . .
C10 C 0.69745(12) 0.14001(12) 0.80197(10) 0.0211(3) Uani 1 1 d . . .
C26 C 0.96605(12) 0.25267(12) 0.73499(10) 0.0238(3) Uani 1 1 d . . .
C16 C 0.77644(12) 0.23661(12) 1.06544(10) 0.0215(3) Uani 1 1 d . . .
C7 C 0.83522(11) 0.06631(11) 0.96684(10) 0.0192(3) Uani 1 1 d . . .
H7 H 0.9077 0.0669 1.0041 0.023 Uiso 1 1 calc R . .
C28 C 1.03334(13) 0.37770(13) 0.86551(12) 0.0299(4) Uani 1 1 d . . .
H28 H 1.0812 0.4352 0.8868 0.036 Uiso 1 1 calc R . .
C27 C 1.03946(13) 0.34096(13) 0.77234(12) 0.0311(4) Uani 1 1 d . . .
H27 H 1.0920 0.3721 0.7291 0.037 Uiso 1 1 calc R . .
C22 C 0.71362(12) 0.38315(13) 1.17767(11) 0.0253(3) Uani 1 1 d . . .
H22 H 0.7341 0.3361 1.2313 0.030 Uiso 1 1 calc R . .
C13 C 0.50185(13) 0.13833(13) 0.77088(11) 0.0282(3) Uani 1 1 d . . .
H13 H 0.4402 0.1268 0.7272 0.034 Uiso 1 1 calc R . .
C23 C 0.95424(12) 0.33166(12) 0.93683(11) 0.0227(3) Uani 1 1 d . . .
C12 C 0.60809(12) 0.11993(12) 0.73808(11) 0.0247(3) Uani 1 1 d . . .
H12 H 0.6195 0.0938 0.6725 0.030 Uiso 1 1 calc R . .
C6 C 0.85379(12) 0.02115(12) 0.85928(10) 0.0218(3) Uani 1 1 d . . .
H6 H 0.9343 0.0066 0.8511 0.026 Uiso 1 1 calc R . .
C14 C 0.48602(12) 0.17359(13) 0.86758(12) 0.0282(3) Uani 1 1 d . . .
H14 H 0.4130 0.1831 0.8905 0.034 Uiso 1 1 calc R . .
C5 C 0.76015(12) -0.02265(12) 1.01282(10) 0.0219(3) Uani 1 1 d . . .
H5 H 0.7165 0.0022 1.0710 0.026 Uiso 1 1 calc R . .
C17 C 0.72805(12) 0.34853(12) 1.07955(11) 0.0221(3) Uani 1 1 d . . .
C11 C 0.81507(12) 0.10949(12) 0.78086(10) 0.0213(3) Uani 1 1 d . . .
H11 H 0.8243 0.0841 0.7107 0.026 Uiso 1 1 calc R . .
C15 C 0.57554(12) 0.19532(12) 0.93188(11) 0.0238(3) Uani 1 1 d . . .
H15 H 0.5638 0.2198 0.9980 0.029 Uiso 1 1 calc R . .
C18 C 0.69769(14) 0.41868(13) 1.00186(12) 0.0297(3) Uani 1 1 d . . .
H18 H 0.7078 0.3965 0.9349 0.036 Uiso 1 1 calc R . .
C4 C 0.79125(13) -0.08898(12) 0.85904(11) 0.0263(3) Uani 1 1 d . . .
H4 H 0.7731 -0.1189 0.7913 0.032 Uiso 1 1 calc R . .
C2 C 0.83657(13) -0.12169(12) 1.03350(11) 0.0266(3) Uani 1 1 d . . .
H2A H 0.7997 -0.1772 1.0750 0.032 Uiso 1 1 calc R . .
H2B H 0.9063 -0.0986 1.0673 0.032 Uiso 1 1 calc R . .
C3 C 0.69073(13) -0.06860(12) 0.92421(11) 0.0259(3) Uani 1 1 d . . .
H3A H 0.6510 -0.1368 0.9410 0.031 Uiso 1 1 calc R . .
H3B H 0.6388 -0.0140 0.8951 0.031 Uiso 1 1 calc R . .
C1 C 0.85829(14) -0.16701(13) 0.92725(12) 0.0311(4) Uani 1 1 d . . .
H1A H 0.9379 -0.1643 0.9122 0.037 Uiso 1 1 calc R . .
H1B H 0.8318 -0.2434 0.9202 0.037 Uiso 1 1 calc R . .
C19 C 0.65289(16) 0.52066(15) 1.02165(13) 0.0397(4) Uani 1 1 d . . .
H19 H 0.6317 0.5679 0.9683 0.048 Uiso 1 1 calc R . .
C20 C 0.63908(16) 0.55360(15) 1.11945(15) 0.0431(4) Uani 1 1 d . . .
H20 H 0.6083 0.6235 1.1331 0.052 Uiso 1 1 calc R . .
C21 C 0.66993(14) 0.48503(14) 1.19717(13) 0.0346(4) Uani 1 1 d . . .
H21 H 0.6610 0.5081 1.2641 0.042 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C23 1.2191(18) . ?
O1 C26 1.2202(18) . ?
O3 C16 1.2134(17) . ?
C25 C24 1.346(2) . ?
C25 C26 1.482(2) . ?
C25 C11 1.503(2) . ?
C9 C15 1.390(2) . ?
C9 C10 1.3973(19) . ?
C9 C8 1.5353(19) . ?
C8 C24 1.5342(19) . ?
C8 C16 1.5388(19) . ?
C8 C7 1.5861(19) . ?
C24 C23 1.484(2) . ?
C10 C12 1.387(2) . ?
C10 C11 1.505(2) . ?
C26 C27 1.477(2) . ?
C16 C17 1.500(2) . ?
C7 C5 1.5530(19) . ?
C7 C6 1.5667(19) . ?
C28 C27 1.332(2) . ?
C28 C23 1.481(2) . ?
C22 C21 1.379(2) . ?
C22 C17 1.398(2) . ?
C13 C14 1.385(2) . ?
C13 C12 1.388(2) . ?
C6 C4 1.543(2) . ?
C6 C11 1.571(2) . ?
C14 C15 1.396(2) . ?
C5 C2 1.544(2) . ?
C5 C3 1.546(2) . ?
C17 C18 1.392(2) . ?
C18 C19 1.386(2) . ?
C4 C3 1.536(2) . ?
C4 C1 1.540(2) . ?
C2 C1 1.558(2) . ?
C19 C20 1.387(3) . ?
C20 C21 1.382(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C24 C25 C26 122.19(13) . . ?
C24 C25 C11 115.58(12) . . ?
C26 C25 C11 122.15(12) . . ?
C15 C9 C10 119.46(13) . . ?
C15 C9 C8 126.44(13) . . ?
C10 C9 C8 113.41(12) . . ?
C24 C8 C9 107.83(11) . . ?
C24 C8 C16 113.55(11) . . ?
C9 C8 C16 114.86(11) . . ?
C24 C8 C7 103.42(10) . . ?
C9 C8 C7 105.40(11) . . ?
C16 C8 C7 110.85(11) . . ?
C25 C24 C23 120.06(13) . . ?
C25 C24 C8 114.08(12) . . ?
C23 C24 C8 125.29(12) . . ?
C12 C10 C9 120.98(13) . . ?
C12 C10 C11 124.61(13) . . ?
C9 C10 C11 114.07(12) . . ?
O1 C26 C27 121.99(14) . . ?
O1 C26 C25 121.10(14) . . ?
C27 C26 C25 116.90(13) . . ?
O3 C16 C17 119.78(13) . . ?
O3 C16 C8 119.18(13) . . ?
C17 C16 C8 121.02(12) . . ?
C5 C7 C6 102.60(11) . . ?
C5 C7 C8 117.93(11) . . ?
C6 C7 C8 109.76(11) . . ?
C27 C28 C23 122.02(14) . . ?
C28 C27 C26 121.21(14) . . ?
C21 C22 C17 120.54(15) . . ?
C14 C13 C12 119.79(14) . . ?
O2 C23 C28 120.43(14) . . ?
O2 C23 C24 122.32(13) . . ?
C28 C23 C24 117.21(13) . . ?
C10 C12 C13 119.41(14) . . ?
C4 C6 C7 103.16(11) . . ?
C4 C6 C11 117.22(12) . . ?
C7 C6 C11 109.24(11) . . ?
C13 C14 C15 121.10(14) . . ?
C2 C5 C3 99.66(12) . . ?
C2 C5 C7 105.36(11) . . ?
C3 C5 C7 105.11(11) . . ?
C18 C17 C22 118.92(14) . . ?
C18 C17 C16 124.23(13) . . ?
C22 C17 C16 116.85(13) . . ?
C25 C11 C10 107.40(12) . . ?
C25 C11 C6 103.60(11) . . ?
C10 C11 C6 108.23(11) . . ?
C9 C15 C14 119.13(14) . . ?
C19 C18 C17 120.42(15) . . ?
C3 C4 C1 100.10(12) . . ?
C3 C4 C6 104.67(12) . . ?
C1 C4 C6 106.58(12) . . ?
C5 C2 C1 103.08(12) . . ?
C4 C3 C5 94.18(11) . . ?
C4 C1 C2 103.14(12) . . ?
C18 C19 C20 119.87(16) . . ?
C21 C20 C19 120.19(16) . . ?
C22 C21 C20 120.06(15) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.06
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.046
_database_code_depnum_ccdc_archive 'CCDC 983252'
